CN106751568B - A kind of antibacterial PBAT/PLA composite membranes and preparation method thereof - Google Patents
A kind of antibacterial PBAT/PLA composite membranes and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to PBAT/PLA, and capacity increasing technique field is blended, and in particular to a kind of antibacterial PBAT/PLA composite membranes, including following component and part is：98 parts of PBAT/PLA94,0.5 2 parts of antibiotic property bulking agent, 0.5 2 parts of butyl titanate, 12 parts of lubricant, each component and parts by weight are in wherein PBAT/PLA：40 parts of 80 parts of PBAT60, PLA20.A kind of antibacterial PBAT/PLA composite membranes provided by the invention, after antibiotic property bulking agent and butyl titanate are added in PBAT/PLA co-mixing systems, the compatibility of system can not only be made to be greatly improved, also it is avoided that the additives such as light stabilizer and the antiseptic of addition low molecular weight, lower-molecular substance is effectively prevented to permeate during materials'use and storage, transport phenomena, the problem of finally material property being made to decline.
Description
Technical field
The present invention relates to PBAT/PLA, and capacity increasing technique field is blended, and in particular to a kind of antibacterial PBAT/PLA composite membranes and its
Preparation method.
Background technology
With the high speed development of national economy, the use of high molecular material has penetrated into the every field of people's life,
It brings great convenience to our life.However, common high molecular material is difficult to biodegradation due to most of, thus lead
Serious problem of environmental pollution is caused, such as " white pollution ".The highest attention to environmental problem and quality of life along with people
It is required that raising, exploitation totally biodegradable high molecular material have become domestic and international research hotspot now.
Polylactic acid (polylactic acid, PLA) is the shallow lake extracted by renewable plant resources such as corn, potatos
Powder is converted into glucose, and glucose becomes lactic acid, the aliphatic polyester being further polymerized by fermentation.The vitrifying of PLA
About 180 DEG C of about 55 DEG C of transition temperature Tg, fusing point Tm, there is a good biocompatibility, and can complete biodegradable, drop
Final product after solution is water and carbon dioxide (CO2), thus, it is nontoxic, environmental pollution will not be caused.Meanwhile the stretching of PLA is strong
Degree, compression modulus are high, the transparency is good；Processing and forming is convenient, can be as the synthesis macromolecules such as PP, PS and PET general
It squeezed out, be molded on process equipment, blowing the processing and formings such as bottle, thermoforming to produce film, sheet material, bottle and various thermoformings
Product and injection moulded products.In short, PLA is not only environmental-friendly, is widely used, can also be reduced to non-renewable resources stone from its source
The consumption of oil, has the title of " green plastic " good reputation, causes the broad interest of people.But the shortcomings that PLA, is mainly shown as matter
Hard and crisp, impact resistance, hydrophily are poor, and degradation cycle is difficult to control.This is greatly limited their application, and is especially led in packaging
Domain.Therefore, PLA is modified to for research hotspot, particularly in terms of toughening modifying.
Biodegradated polymer materal polyadipate butylene terephthalate (PBAT) has good flexibility, with
PLA is all thermoplastic, can be processed using common plastic working method.In view of the complementation of performance between the two
Property, select PBAT to be blended with PLA, the high polymer alloy of preparation not only has good toughness, while not losing its biology again can
Degradability.
But PLA/PBAT alloys are an incompatible two-phase system, dispersed phase PBAT will be dispersed in greater particle size
In PLA matrixes, this will greatly limit PBAT to PLA toughness improvements.The compatibility for thus needing both raisings, makes PBAT
It is more obvious to the toughening effect of PLA, to obtain the material that performance is more preferable, more stable.
Capacity increasing modifying, both modified compatibility are carried out to PLA/PBAT alloys using polyethylene glycol (PEG) bulking agent
Different degrees of raising is all obtained, but still cannot achieve the effect that satisfied, the stability of material is poor, and lower-molecular substance exists
It is easily permeated during materials'use and storage, transport phenomena finally makes material property decline.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to a kind of antibacterial PBAT/PLA composite membranes be provided, by antibacterial
After property bulking agent and butyl titanate are added in PBAT/PLA co-mixing systems, can not only make the compatibility of system obtain compared with
Big raising, moreover it is possible to avoid the additives such as light stabilizer and the antiseptic of addition low molecular weight, effectively prevent lower-molecular substance
The problem of being permeated during materials'use and storage, transport phenomena, finally material property being made to decline.
To achieve the purpose of the present invention, the present invention adopts the following technical scheme that：
A kind of antibacterial PBAT/PLA composite membranes, including following component and part is：
Each component and parts by weight are in wherein PBAT/PLA：
60-80 parts of PBAT
20-40 parts of PLA.
Specifically, above-mentioned antibiotic property bulking agent is：
Wherein, R is-CH3Or-CH2CH3。
The preparation method of above-mentioned antibacterial bulking agent includes the following steps：
Step 1：It is 1 by molar ratio:2 polyethylene glycol (PEG4000) and phthalic anhydride is added to reaction vessel
In, it is uniformly mixed, is warming up to 66-70 DEG C, and it is reaction system that the concentrated sulfuric acid for the 2wt% that weight is reaction system and weight, which is added,
0.3wt% p-hydroxyanisole, after phthalic anhydride thawing after, be warming up to 80 DEG C, continue stir 6h after, be cooled to
Room temperature with ether precipitated product, then is washed, and is filtered, dry, obtains first generation product, structural formula is：
Step 2：It is 1 by molar ratio:2 first generation product and dihydric alcohol containing hindered amine group are added in reaction kettle, mix
The tetrabutyl titanate that the 4wt% that weight is reaction system is uniformly added is closed, and is heated to 250 DEG C, reacts 6 hours, is cooled to room
Temperature with ether precipitated product, then is washed, and is filtered, dry, obtains second generation product, structural formula is：
The structural formula of dihydric alcohol containing hindered amine group is：
Step 3：It is 1 by molar ratio:2 second generation product and phthalic anhydride is added in reaction vessel, and mixing is equal
It is even, it is warming up to 66-70 DEG C, and the concentrated sulfuric acid for the 2wt% that weight is reaction system is added and 0.2wt% that weight is reaction system
P-hydroxyanisole, after phthalic anhydride thawing after, be warming up to 80-85 DEG C, continue stir 6h after, be cooled to room temperature, use
Ether precipitated product, then wash, it filters, it is dry, third generation product is obtained, structural formula is：
Step 4：It is 1 by molar ratio:2 third generation product and 2- amino -3- pyridones is added in reaction kettle, mixing
Uniformly, the antimony glycol for the 3wt% that weight is reaction system is added, and is heated to 260 DEG C, reacts 2 hours, is cooled to room temperature,
It with ether precipitated product, then washs, filters, it is dry, forth generation product is obtained, structural formula is：
Its infrared test result is as follows：
FTIR(KBr)：N-H2Stretching vibration peak 3410cm-1, pyridine characteristic peak 1600cm-1And 1570cm-1,-COO features
Peak 1740cm-1And 1300cm-1, phenyl ring characteristic peak 1580cm-1,-CH2 characteristic peaks 1390cm-1, C-O-C characteristic peaks 1070cm-1,
C-N characteristic peaks 1280cm-1。
Nuclear magnetic spectrogram as shown in Figure 1, nuclear-magnetism test result is as follows：
1H-NMR (400MHz, DMSO-d6) δ 8.18-8.24 (p, 4H), 8.08-8.10 (n, 4H), 7.87 (m, 2H),
7.68-7.71 (l, 4H), 7.58 (k, 4H), 7.07 (j, 2H), 6.75 (i, 2H), 4.88 (h, 2H), 4.67 (g, 4H), 4.00
(f, 4H), 3.79 (e, 4H), 2.85 (d, 2H), 2.27 (c, 6H), 2.24 (b, 4H), 1.63 (a, 8H).
Specifically, above-mentioned lubricant is in stearic acid, aluminum stearate, calcium stearate, zinc stearate or tristerin
One kind.
Specifically, the weight average molecular weight of above-mentioned PLA is 6-8 ten thousand.
Specifically, the weight average molecular weight of above-mentioned PBAT is 6-10 ten thousand.
A kind of preparation method of antibacterial PBAT/PLA composite membranes, includes the following steps：
(1) raw material is weighed by the parts by weight of above-mentioned each component, and by PLA particles and PBAT particles in vacuum drying chamber
Dry 3-5h at 70 DEG C；
(2) PLA particles, PBAT particles, antibiotic property bulking agent, butyl titanate and the lubricant after drying are mixed in proportion
Double screw extruder is added to after closing uniformly and carries out extruding pelletization, and the temperature in each area of setting extruder is according between 170-185 DEG C；
(3) the PBAT/PLA blended particles obtained by step (2) are added to blowfilm shaping in plastic film blowing machine, prepared
The temperature of PBAT/PLA composite membranes, the wherein areas inflation film manufacturing machine 1-5 is followed successively by 190 DEG C, 200 DEG C, 200 DEG C, 190 DEG C and 185 DEG C.
The device have the advantages that：
(1) a kind of antibacterial PBAT/PLA composite membranes of the invention, the antibiotic property bulking agent of addition still maintain the soft of PEG
Property strand, can promote PBAT and PLA relatively closely to be arranged with PEG, improve the impact strength, tensile strength and mould of composite material
Amount.
(2) a kind of antibacterial PBAT/PLA composite membranes of the invention, in the antibiotic property bulking agent of addition, PEG strands both ends
The presence of amino can form hydrogen bond, but also the binding force enhancing between two polymer of PLA and PBAT.
(3) a kind of antibacterial PBAT/PLA composite membranes of the invention, in the antibiotic property bulking agent of addition, in PEG strands two
End introduces hindered amine group, pyridine groups and amino, makes the PBAT/PLA that the present invention is added in PBAT/PLA co-mixing systems
There is good photostability and antibiotic property after bulking agent is blended, while the light for also making system avoid addition low molecular weight is stablized
The additives such as agent and antiseptic effectively prevent lower-molecular substance and are permeated during materials'use and storage, and migration is existing
As the problem of finally material property being made to decline.
(4) a kind of antibacterial PBAT/PLA composite membranes of the invention are added to antibiotic property increasing in PBAT/PLA co-mixing systems
Hold agent, there is extraordinary compatibility, the existing good ultraviolet light stability of thin-film material made, which has, keeps good mechanics
Performance.
(5) in a kind of antibacterial PBAT/PLA composite membranes of the invention, butyl titanate is added to as catalyst, can be promoted
Esterification occurs in melt blending into PBAT and PLA, produces PLA-PBAT copolymers to increase the compatibility of two-phase interface
And adhesive attraction；And the addition of butyl titanate effectively increases the light transmittance of antibacterial PBAT/PLA composite membranes again.
Description of the drawings
Fig. 1 is the nuclear magnetic spectrogram of the antibiotic property bulking agent of the present invention.
Specific implementation mode
Presently in connection with embodiment, the present invention is described in further detail.
Embodiment 1
A kind of antibacterial PBAT/PLA composite membranes, including following component and part is：
Each component and parts by weight are in wherein PBAT/PLA：
80 parts of PBAT (molecular weight 80,000)
40 parts of PLA (molecular weight 80,000).
Wherein antibiotic property bulking agent is：
Wherein, R is-CH3Or-CH2CH3。
A kind of preparation method of antibacterial PBAT/PLA composite membranes, includes the following steps：
(1) raw material is weighed by the parts by weight of above-mentioned each component, and by PLA particles and PBAT particles in vacuum drying chamber
Dry 3-5h at 70 DEG C；
(2) PLA particles, PBAT particles, antibiotic property bulking agent, butyl titanate and the lubricant after drying are mixed in proportion
Double screw extruder is added to after closing uniformly and carries out extruding pelletization, and the temperature in each area of setting extruder is according between 170-185 DEG C；
(3) the PBAT/PLA blended particles obtained by step (2) are added to blowfilm shaping in plastic film blowing machine, prepared
The temperature of PBAT/PLA composite membranes, the wherein areas inflation film manufacturing machine 1-5 is followed successively by 190 DEG C, 200 DEG C, 200 DEG C, 190 DEG C and 185 DEG C.
Embodiment 2-7, comparative example 1-3 are with embodiment 1, the difference is that table 1：
Table 1：
The compound film properties tests of antibacterial PBAT/PLA of embodiment 1-7 and comparative example 1-3 are as shown in table 2：
It is enlightenment with above-mentioned desirable embodiment according to the present invention, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to determine its technical scope according to right.
Claims (5)
1. a kind of antibacterial PBAT/PLA composite membranes, including following component and part is：
94-98 parts of PBAT/PLA
0.5-2 parts of antibiotic property bulking agent
0.5-2 parts of butyl titanate
1-2 parts of lubricant；
Each component and parts by weight are in wherein PBAT/PLA：
60-80 parts of PBAT
20-40 parts of PLA；
The antibiotic property bulking agent is：
Wherein, R is-CH3Or-CH2CH3。
2. a kind of antibacterial PBAT/PLA composite membranes as described in claim 1, it is characterised in that：The lubricant be stearic acid,
One kind in aluminum stearate, calcium stearate, zinc stearate or tristerin.
3. a kind of antibacterial PBAT/PLA composite membranes as described in claim 1, it is characterised in that：The weight average molecular weight of the PLA
For 6-8 ten thousand.
4. a kind of antibacterial PBAT/PLA composite membranes as described in claim 1, it is characterised in that：The weight average molecular weight of the PBAT
For 6-10 ten thousand.
5. a kind of preparation method of antibacterial PBAT/PLA composite membranes according to any one of claims 1-4, it is characterised in that packet
Include following steps：
（1）Raw material is weighed by the parts by weight of above-mentioned each component, and by PLA particles and PBAT particles 70 DEG C in vacuum drying chamber
Lower dry 3-5h；
（2）PLA particles, PBAT particles, antibiotic property bulking agent, butyl titanate and lubricant after drying is mixed in proportion
Double screw extruder is added to after even and carries out extruding pelletization, and the temperature in each area of setting extruder is according between 170-185 DEG C；
（3）By step（2）The PBAT/PLA blended particles of gained are added to blowfilm shaping in plastic film blowing machine, prepare PBAT/PLA
The temperature of composite membrane, the wherein areas inflation film manufacturing machine 1-5 is followed successively by 190 DEG C, 200 DEG C, 200 DEG C, 190 DEG C and 185 DEG C.
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| CN112679928A (en) * | 2020-12-28 | 2021-04-20 | 东莞市三至新材料技术有限公司 | Full-biodegradable antibacterial PLA/PBAT film and preparation method thereof |
| CN113265130B (en) * | 2021-05-24 | 2023-05-05 | 李涛 | High-tensile full-biodegradable antibacterial film and preparation method and application thereof |
| CN113429757B (en) * | 2021-07-08 | 2023-03-14 | 东莞市金富亮塑胶科技有限公司 | Biodegradable anti-fogging master batch for mulching film and preservative film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103589124A (en) * | 2012-08-14 | 2014-02-19 | 上海杰事杰新材料(集团)股份有限公司 | Fully-biodegradable PLA/PBAT composite film and making method thereof |
| CN104098880A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | High-performance polylactic acid composite material and preparation method thereof |
| CN104559087A (en) * | 2015-01-21 | 2015-04-29 | 江苏科技大学 | Controllable bio-based full-degradable mulching film |
| CN105273377A (en) * | 2015-07-31 | 2016-01-27 | 邓铁军 | Biodegradable material and preparation method and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589124A (en) * | 2012-08-14 | 2014-02-19 | 上海杰事杰新材料(集团)股份有限公司 | Fully-biodegradable PLA/PBAT composite film and making method thereof |
| CN104098880A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | High-performance polylactic acid composite material and preparation method thereof |
| CN104559087A (en) * | 2015-01-21 | 2015-04-29 | 江苏科技大学 | Controllable bio-based full-degradable mulching film |
| CN105273377A (en) * | 2015-07-31 | 2016-01-27 | 邓铁军 | Biodegradable material and preparation method and use thereof |
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